Apparatus for collecting products of fractionation



y 17, 1956 D. BELTZ EFAL 2,755,008

APPARATUS FOR COLLECTING PRODUCTS OF FRACTIONATION Filed Aug. 10, 1953 2Sheets-Sheet l iTL [Ill a W Mm N IA/VENTORS 0A mu BEL 725 R/c/m/w z; BELTZ A TTORNE V.

y 17, 1956 D. BELTZ ET AL 2,755,008

APPARATUS FOR COLLECTING PRODUCTS OF FRACTIONATION M/VENTOR .5 DANIEL Bar2, w RIC HHRD 551.11

A 7' TORNE K APPARATUS 'FGR CQLLECTING EPRQDUCTS OF FRACTIGNATION DanielBeltz and Richard E. Beltz, -Los Angeles, Calif.

Application August 10, 1953,.Serial No. 373,142

7 Claims. (Cl. 22696) This invention relates in general to an art knownin the realm of science by the broad term chromatography orchromatographic analysis but more specifically practised in industry andthe field .of chemistry and research as fractionation by means of whichcertain components of chemical solutions are separated from a parentcompound through the instrumentality of the chromatographic column.Although fractionation comprehends distillation in the separation ofcertain compounds of petroleum and other compounds by heating andvolatilization the apparatus of our invention has no relation to adistillation process or apparatus, nor do our present improvementsindeed relate to othertypes of fractionation except as a collector forthe products of fractionation, and to such end an important object is toprovide a mechanical unit arranged to support and automatically move aplurality of flasks or containers in single file into and from positionsbeneath a column of a parent fluid in which the separable components tobe collected are resident.

Another object is to provide reliable means for utilizing hydrostaticpressure derived from an elevated volume of water which is conducted inalternate charges to oscillating cups mounted on opposite sides of acommon fulcrum so that the weight of the water-laden cups willalternately swing a common oscillator between charging and emptyingpositions and regulate the extent to which the flask supporting tablemay be rotated under motive power supplied by a gravity actuated weight,or otherwise.

Apparatus for serving the purpose of this invention-at least broadly-hasbeen heretofore used in industry but are too expensive and cumbersomefor use in research laboratories and even small industrial plants.Hence, it is an object to provide an inexpensive unit of low initialcost and maintenance requirements which is of simplified structure andmechanical arrangement and capable of operation by the force of gravityinstead of by costly and complicated electric motors and attendantdevices.

Other and more detailed objects will appear as the descriptionprogresses.

We have shown a preferred form of apparatus embodying the invention inthe accompanying drawings in which:

Fig. 1 is a side elevational view partly in section;

Fig. 2 is an elevational view of the unit as seen from the plane of line2-2, of Fig. 1; v

Fig. 3 is a top plan View; on line 3-3 of Fig. l; and

Figs. 4 and 5 are respectively, sectional elevations on lines 4-4 and 55of Fig. 1.

As shown, the unit includes a suitable supporting frame F withhorizontal member 1, 1 extended longitudinally, transverse members 2, 2and upright members 3, v3 so framed and joined as to provide maximumrigidity. A rotatable table or platform T is supported on frame F bymeans of a vertical shaft 5 which revolves in bearings 4, 4 secured toupper and lower members of the frame.

1 ates atent Table T has a pulley Sat its bottom and affixed to shaftsto which one end of a cable 6 is secured. Said cable runs over an idlerpulley 7 mounted on the frame on a stool 8 and a weight 9 is secured tothe free end of cable 6. Thus, the force of gravity applied to pulley 5tends to rotate pulley 5 and table Tat least throughout one completerevolution of the table but intermittently in step-by-step movementsunder control 'of an escape ment mechanism to be hereinafter described.The upper side of table T has a plurality of depressions 10 therein atuniformly spaced points for :holding flasks or con tainers C in fixedpositions on the table in a-circle concentric with the table orotherwise but in any case so that as the table is fractionally rotatedthe flasks will be advanced in sequence to the same position beneath aseparator column A adapted to contain a compound from which thecompounds are dispensed in a gradual process into the flasks C, oneafter another in succession.

While power for rotating table T is derived from weight 9, theescapement mechanism which regulates rotation of the table and times thesuccessive movement of flasks C to charging position beneath column A isactuated by a simple water motor shown in .Fig. 1 and including a bar 11oscillatably mounted on frame F on a shaft 12 in spaced bearings 13, 13and having similar water receiving cups 14 at opposite ends of the barand equidistant from the axis of shaft 12. Preferably cups 14 are of thesame form, size and capacity soas to hold equal quantities of water andthe depth of the cups .is gradually increased from their inner to theirouter margins. Water is fed to cups 14 alternately as bar 11 isoscillated, from an elevated tank 15, through a tube 16, a needle valve17, a spout 18 and separate filling tubes 19, 19 which have their upperends bend to adjacent positions below spout 18. Said spout is shiftableto alternate positions over the inlets to tubes 19, 19' by means of abar 2% which is pivoted on frame F at 21 and has its upper end afixed tospout 18 and its lower end hinged at 22 to a collar 23 on shaft 12.Hence, as the leftmost cup 14 (Fig. 2) is swung upwardly with shaft 12and the rightmostcup swung downwardly, and vice versa, the

spout 18 will be swung into position over the tube 19 associated withthe raised cup while the water will be discharged from the downmost cup.The member 23 is tensioned as by means of a pair of tension springs 24,24 secured at their upper ends'to opposite ends of a. bar 25 which islinked at 26 to member 23, While the lower ends of springs 24 areanchored to the base of frame F as shown in Fig. 5. Thus, as shaft 12and cups 14 are oscillated in opposite directions the springs 24 urgedthem to an opposite extreme of movement.

Rotation of table T is arrested and limited each time a cup 14 is raisedto charging position, by one of a pair of vertical stop rods 27, 27which are slidable in spaced guides 28 and 29 on the frame. Said rods 27have similar loops 27a, 27a with elongated openings 27b, 27b thereinthrough which opposite end portions of a rod 30 extends. Rod 36 isafiixed at an intermediate point to and is oscillated by shaft 12 andthe rod 30 alternately raises and lowers rods 27 into the path of radialpins 31 borne by and extended from the edge of table T in line with eachflask seat 19. As the table is moved a flask C is positioned belowcolumn A all of an accumulated component as at a in Fig. 1 has beenprecipitated from the solution a and discharged through an outlet 31under control of a valve 32, or at least until valve 32 is closed by anattendant but in every case until a cup 14 has been filled with waterfrom tank 15 and overbalan'ces shaft 12 so as to rotate said shaft andrelease the stop rod 27 which up to that point had restrained the tablefrom further operation. Other operations may follow for movingsuccessive flasks to filling position with the same or a differentseparable components a and the compound fluid a vary and their rate ofprecipitation, settling and flow varies from a very slow drip upwardly,due to inherent properties and both physical and chemicalcharacteristics. All components a as well as the compound a areintroduced to column A through an inlet 33. Colum A may have a body 34of glass or other suitable material with inserted end closures 35 and 36bearing the outlet 31 and inlet 33, respectively.

Water is delivered to tank 15 through a pipe 15a and a level of water ismaintained in the tank by means of an overflow pipe 15b. Needle valve 17controls flow of water by gravity from spout 18 into tubes 19 anddischarge of water in proper volume into cups 14 of oscillator 11.

Essentially, therefore, this invention comprehends the provision of anautomatically operable apparatus which includes a platform or tablearranged to support a plurality of flasks in fixed position forintermittent and successive movement to a common position whereat theymay be filled in whole or in part with components of a compound solutionfrom a relatively elevated container, a suitable means for moving thetable and flasks, and a water driven mechanism for timing the movementof the platform or table, whereby the components of a solution may beseparately collected in dilferent flasks at a minimum cost and in acontinuing operation.

We claim:

1. An apparatus for collecting fractions from compounds comprising: aframe, a table rotatably mounted thereon, means constantly urgingunidirectional rotation of said table, a container supported in fixedposition above a plurality of flasks borne by said table and adapted tohold a column of liquid, a water motor including a receptacle forholding a static volume of water, and an oscillator having cupsequidistant from its axis, means for alternately discharging water fromsaid receptacle into said cups as said oscillator is reversely swung onits axis, stop devices on said table corresponding in position to theflasks on the table, and means movable on said frame operativelyconnected with said oscillator for movement into engagement with saidstop devices as the table is fractionally rotated to place a flask inposition below said container in timed relation to said oscillator,whereby different components of the liquid in said container may bedischarged into separate flasks as the table is successively rotated.

2. An apparatus as set forth in claim 1 wherein said means foralternately discharging water includes a dis charge pipe leading fromsaid water receptacle to a point of discharge, separate conduits havinginlets adjacent said point of water discharge and outlets disposed abovesaid cups when the cups are at their uppermost positions, and aconnection to said oscillator for shifting said discharge pipe toalternately discharge water into said cups and thereby effectoscillation of said oscillator.

3. An apparatus as set forth in claim 1 wherein said means foralternately discharging water includes a discharge pipe leading fromsaid water receptacle to a point of discharge, separate conduits havinginlets disposed adjacent said point of water discharge and outletsdisposed above said cups when the cups are at their uppermost positions,and a connection to said oscillator for rocking said discharge pipeabout its axis to alternately distribute water to said conduits.

4. An apparatus for collecting fractions from compounds comprising: aframe, a table rotatably mounted thereon, means constantly urgingunidirectional rotation of said table, a container supported in fixedposition above a plurality of flasks borne by said table and adapted tohold a column of liquid, a water motor including a receptacle forholding a static volume of water, and an oscillator having cupsequidistant from its axis, means for alternately discharging water fromsaid receptacle into said cups as said oscillator is reversely swung onits axis, stop devices on said table corresponding in position to theflasks on the table, and means movable on said frame operativelyconnected with said oscillator for movement into engagement with saidstop devices as the table is fractionally rotated to place a flask inposition below said container in timed relation to said oscillator,whereby different components of the liquid in said container may bedischarged into separate flasks as the table is successively rotated,said movable means including a bar cooscillatable with and by saidoscillator, said bar having retaining means at its opposite endsengagcable with said stop devices to time the fractional rotation of thetable with the movement of said oscillator.

5. An apparatus for collecting fractions from compounds comprising: aframe, a table rotatably mounted thereon, means constantly urgingunidirectional rotation of said table, a container supported in fixedposition above a plurality of flasks borne by said table and adapted tohold a column of liquid, a water motor including a receptacle forholding a static volume of water and a oscillator having cupsequidistant from its axis, means for alternately discharging water fromsaid receptacle into said cups as said oscillator is reversely swung onits axis, stop devices on said table corresponding in position to theflasks on the table, and means movable on said frame operativelyconnected with said oscillator for movement into engagement with saidstop devices as the table is fractionally rotated to place a flask inposition below said container in timed relation to said oscillator,whereby different components of the liquid in said container may bedischarged into separate flasks as the table is successively rotated,and means for supplying desired elements to and for discharging the samefrom said container into said flasks.

6. An apparatus for collecting fractions from compounds comprising: aframe, an upright shaft journaled thereon, a table secured to the upperend of said shaft, a pulley on said shaft below said table, means forrotating said pulley, means on said table for supporting a plurality offlasks in uniformly spaced positions on said table, a containersupported above said flasks at a fixed point for holding a liquid fromwhich fractions may be discharged selectively into said flasks as thetable is fractionally rotated to position successive flasks under anoutlet to said container, stop devices borne by and extended from theflask position on said table and cooperating stops movable on said frameat timed intervals, an oscillator rockably supported on said frame andhaving cups equidistant from its axis, a receptacle for water, adischarge pipe leading from said receptacle to a point of alternatedischarge into said cups and having a discharge spout at said point, apair of oppositely extended conduits having inlets adjacent said pointof discharge and outlets above the uppermost positions of said cups,means operatively connecting said oscillator with and for shifting saidspout to alternate positions above said conduits, and means operativelyconnecting said slidable stop devices with said oscillator for stoppingrotation of said table at regularly timed intervals as the contents ofsaid container are discharged into said flasks in succession.

7. An apparatus for collecting fractions from compounds comprising: acontainer stationarily supported for holding a column of liquidcontaining fractions to be collected, a table movably supported belowsaid container and arranged to hold a plurality of flasks in uniformlyspaced positions for successive movement to a common position below anoutlet of said container, means drivingly connected with said table formoving the table and flasks in a given direction and plane beneath saidcontainer, and a separately actuated mechanism for arresting movement ofsaid table at uniformly timed intervals while the flasks are receivingfractions from said container, said arresting mechanism including anoscillator having cups supported at opposite sides of its axis andcooperating stop devices associated with said table and with saidoscillator, an elevated Water tank having a spout for controllingdischarge of water from said tank, a pair of spaced tubes having inletsdisposed in a plane below said spout means controlled by said oscillatorfor alternately shifting said spout to positions over the inlets attimes when said cups are moved into positions below outlets to saidtubes, thereby alternatively weighting said cups to the overbalancing ofthe oscillator in opposite direcv tions.

References Cited in the file of this patent UNITED STATES PATENTS2,604,248 Gorham July 22, 1952

1. AN APPARATUS FOR COLLECTING FRACTIONS FROM COMPOUNDS COMPRISING: AFRAME, A TABLE ROTATABLY MOUNTED THEREON, MEANS CONSTANTLY URGINGUNIDIRECTIONAL ROTATION OF SAID TABLE, A CONTAINER SUPPORTED IN FIXEDPOSITION ABOVE A PLURALITY OF FLASKS BORNE BY SAID TABLE AND ADAPTED TOHOLD A COLUMN OF LIQUID, A WATER MOTOR INCLUDING A RECEPTACLE FORHOLDING A STATIC VOLUME OF WATER, AND AN OSCILLATOR HAVING CUPSEQUIDISTANT FROM ITS AXIS, MEANS FOR ALTERNATELY DISCHARGING WATER FROMSAID RECEPTACLE INTO SAID CUPS AS SAID OSCILLATOR IS REVERSELY SWUNG ONITS AXIS, STOP DEVICES ON SAID TABLE CORRESPONDING IN POSITION TO THEFLASKS ON THE TABLE, AND MEANS MOVABLE ON SAID FRAME OPERATIVELYCONNECTED WITH SAID OSCILLATOR FOR MOVEMENT INTO ENGAGEMENT WITH SAIDSTOP DEVICES AS THE TABLE IS FRACTIONALLY ROTATED TO PLACE A FLASK INPOSITION BELOW SAID CONTAINER IN TIMED RELATION TO SAID OSCILLATOR,WHEREBY DIFFERENT COMPONENTS OF THE LIQUID IN SAID CONTAINER MAY BEDISCHARGED INTO SEPARATE FLASKS AS THE TABLE IS SUCCESSIVELY ROTATED.